CN102616867B - Method for extracting and preparing nickel carbonate, nickel sulfate and red ferric oxide from serpentine and tailings thereof - Google Patents
Method for extracting and preparing nickel carbonate, nickel sulfate and red ferric oxide from serpentine and tailings thereof Download PDFInfo
- Publication number
- CN102616867B CN102616867B CN 201210103812 CN201210103812A CN102616867B CN 102616867 B CN102616867 B CN 102616867B CN 201210103812 CN201210103812 CN 201210103812 CN 201210103812 A CN201210103812 A CN 201210103812A CN 102616867 B CN102616867 B CN 102616867B
- Authority
- CN
- China
- Prior art keywords
- filtrate
- filter cake
- nickel
- serpentine
- hour
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for extracting and preparing nickel carbonate, nickel sulfate and red ferric oxide from serpentine and tailings thereof. The serpentine and tailings thereof are used as raw materials. The method comprises the following unit processes of: pre-treating; performing acid leaching; performing fractional precipitation; performing ammonia leaching; acidifying; preparing nickel carbonate; preparing nickel sulfate; and calcining. According to the method, useful components such as nickel and iron in the serpentine can be fully and effectively utilized, products such as nickel carbonate, nickel sulfate and red ferric oxide with tight market demand can be produced, and higher nickel and iron recovery rate can be obtained. The purity of the nickel carbonate is 47.93 percent in terms of nickel and the yield is 90.10 percent; the purity of the nickel sulfate is 22.12 percent in terms of nickel and the yield is 85.73 percent; and the purity of the red ferric oxide is 92.40 percent in terms of Fe2O3 and the yield is 92.94 percent.
Description
One, technical field
The present invention relates to a kind of method of from serpentine, extracting nickel and iron, specifically a kind of by extracting the method for preparing nickelous carbonate, single nickel salt and red iron oxide in serpentine and the mine tailing thereof.
Two, technical background
Serpentine (chemical formula Mg
3[Si
2O
3] (OH)
4) be a kind of at the abundant natural magnesium silicate minerals that contains of China's storage, main component is MgO and SiO
2, also contain minor N iO, Fe
2O
3Deng.In the serpentine ore exploitation and the course of processing, can produce a large amount of mine tailings,, can cause serious environmental to pollute and the wasting of resources if be not used.Analytical results shows that the chemical constitution of serpentine tailing is close with its raw ore.For a long time, people have paid close attention to the utilization research of silicon, magnesium in serpentine and the mine tailing thereof, as utilize the silicon in serpentine and the mine tailing thereof to produce silicon series product such as industrial liquid water glass, white carbon black, metasilicate pentahydrate sodium, silicoorganic compound, utilize the magnesium in serpentine and the mine tailing thereof to produce magnesium series product such as industrial light magnesium oxide, magnesium basic carbonate, magnesium hydroxide.But to the oxide compound of non-ferrous metal such as the nickel that contains in serpentine and the mine tailing thereof and iron etc., research both at home and abroad is also less relatively at present.Along with the continuous consumption and the minimizing of higher-grade nickel ore resource in the world, and both at home and abroad to the continuous increase of nickel product demand, extracting nickel resources from nickeliferous lower ore such as serpentine and mine tailing thereof has become the focus that the lot of domestic and foreign investigator pays close attention to.Therefore, in comprehensive utilization serpentine and mine tailing thereof in silicon, the magnesium, compositions such as wherein nickel of high efficiente callback, iron can not only effectively be avoided the waste of resource, but also it can be turned waste into wealth, and obtain good economic benefit.
In recent years, recycling at nickel in the serpentine and iron has proposed certain methods, being mainly acidleach follows the example of, wherein representational method has: it is that the full wet method of raw material is produced gas-phase silica, transparent magnesiumcarbonate, activated magnesia, single nickel salt with the serpentine that (1) Dai Yuanning has proposed a kind of, and reclaim iron, chromium is the chemical industry metallurgical technology of concentrate.This method sulfuric acid is leaching agent, is promoting agent with halogenide, makes the silicon in the serpentine become the gas phase halide mode to decompose effusion, makes the gas-phase silica product through the ammonium oxidation again.Allow magnesium, iron, nickel, the chromium of leaching become sulphate form to enter solution, remove the impurity fine chrome mine through once alkalization precipitation, the double alkalisation precipitation removes the impurity iron concentrate, and three times sulfide precipitation transforms the system single nickel salt, and four carbonizations precipitation transforms transparent magnesiumcarbonate of system and activated magnesia; The hydrogen sulfide that the heavy nickel reactant of acidolysis sulfuration is emitted is absorbed as sodium sulphite with caustic soda and returns heavy nickel and recycle; The mother liquor ammonium sulfate condensing crystal of the heavy magnesium of carbonization becomes byproduct industrial sulphuric acid ammonium.(2) employing hydrochloric acid such as Zheng Hua leaches serpentine as leaching agent; sulfuric acid leaching filtrate of serpentine is after hydrogen peroxide preoxidation; by stage treatment technology; under constantly stirring, add a certain amount of calcium hydroxide; control pH value; obtain the mixed sediment of ironic hydroxide and aluminium hydroxide, after excessive sodium hydroxide was removed aluminium hydroxide, the oven dry calcining obtained the red iron oxide product.The precipitation filtrate collection is used to prepare magnesium oxide, and the acidleach filter residue is used to prepare porous silica.
By as can be seen above-mentioned, nickel, iron utilize that method exists that technical process complexity, equipment material are had relatively high expectations, the raw materials consumption amount is big, produce problem such as toxic gas hydrogen sulfide in the production process in the existing serpentine.
Three, summary of the invention
The present invention aims to provide a kind of by extracting method prepare nickelous carbonate, single nickel salt and red iron oxide in serpentine and the mine tailing thereof, technical problem to be solved provides and a kind ofly reclaims that purity is higher, recovery method simply and the method for environmental protection from serpentine, extract nickel and ferro element.
Technical solution problem of the present invention adopts following technical scheme:
The present invention is by extracting the method for preparing nickelous carbonate, single nickel salt and red iron oxide in serpentine and the mine tailing thereof, with serpentine and mine tailing thereof is raw material, comprise that pre-treatment, acidleach, fractional precipitation, ammonia soak, the preparation of the preparation of acidifying, nickelous carbonate, single nickel salt and calcine each unit process, it is characterized in that:
Described pre-treatment is serpentine or its mine tailing to be milled to particle diameter obtain powder less than 200 μ m;
Described acidleach is the sulphuric acid soln that adds powder quality 2-10 mass concentration 10-50wt% doubly in described powder, reacted 3-5 hour down at 60-100 ℃, filtering separation is collected filtrate and filter cake, described filter cake is washed with water to neutrality obtains filter cake I, washings and the merging of described filtrate are obtained filtrate I; Described filter cake I can be used for preparing the silicon series product;
Described fractional precipitation is to add lye pH adjustment value 3.0-4.0 in described filtrate I, in 50-90 ℃ of reaction 3-5 hour, reaction finishes after-filtration separated and collected filtrate and filter cake, filter cake is washed with water to neutrality obtains filter cake II, with washings and described filtrate merge filtrate II; Described filter cake II obtained the red iron oxide presoma after under 105-110 ℃ dry 2-4 hour; In described filtrate II, add lye pH adjustment value 7.0-8.5, room temperature-45 ℃ following reaction 2-4 hour, the still aging 3-6 of preserving heat after reaction ends hour, filtering separation is collected filtrate and filter cake, filter cake washing is obtained filter cake III to neutrality, merge washings and filtrate and obtain filtrate II I, filtrate II I can be used for preparing the magnesium series product; Described alkali lye is selected from ammoniacal liquor, sodium hydroxide or potassium hydroxide etc.;
It is to add described filter cake III quality 3-5 times the ammoniacal liquor and the mixing solutions of bicarbonate of ammonia in described filter cake III that described ammonia soaks, at room temperature-90 ℃ following reaction 0.5-3 hour, NH in the mixing solutions of described ammoniacal liquor and bicarbonate of ammonia
3Concentration 4-6mol/L, NH
4HCO
3Concentration 4-6mol/L; React and finish after-filtration collection filtrate and filter cake, the mixing solutions of filter cake with described ammoniacal liquor and bicarbonate of ammonia washed to obtaining filter cake IV with dimethylglyoxime solution detection non-nickle ion, collect washings and filtrate and obtain filtrate IV; Filter cake IV is back to the acidleach operation;
Described acidifying is to add sulfuric acid to destroy the nickel ammine structure in described filtrate IV, and nickel is existed in solution with the ionic state form, and the vitriolic addition takes off with the blueness (color of nickel ammine) that just makes filtrate IV and is as the criterion.Carbonic acid gas can be recycled after absorbing processing.
The preparation of described nickelous carbonate is the pH to 8-9.5 that regulates the filtrate IV after the acidifying with the carbonate solution of mass concentration 5-15wt%, 70-90 ℃ of reaction 0.5-3 hour down, filter back gained filter cake 105-110 ℃ dry 2-4 hour down, promptly obtain nickelous carbonate; Filtrate is back to acidification step and recycles; Described carbonate is selected from yellow soda ash, salt of wormwood etc.;
The preparation of described single nickel salt is the sulphuric acid soln dissolving of the nickelous carbonate of preparation being used mass concentration 5-10wt%, and control reaction end pH value 3-4 is concentrated into density 11-1.3g/cm
3Postcooling leaves standstill after-filtration to room temperature, and the gained filter cake was descended dry 5-10 hour at 30-40 ℃, promptly obtains single nickel salt, and filtrate is back to the nickelous carbonate preparation process and recycles.
Described calcining is that described red iron oxide presoma was calcined 1-3 hour down in 600-800 ℃, promptly gets red iron oxide.
Each step reaction equation of the inventive method is:
A, acidleach
3MgO·2SiO
2·2H
2O+3H
2SO
4→3MgSO
4+2SiO
2·nH
2O+(5-2n)H
2O
Fe
2O
3+3H
2SO
4→Fe
2(SO
4)
3+3H
2O
FeO+H
2SO
4→FeSO
4+H
2O
NiO+H
2SO
4→NiSO
4+H
2O
B, fractional precipitation
Fe
3++ 3OH
-→ α-FeO (OH) ↓+H
2O (a step precipitation)
4Fe
2++ 8OH
-+ 2H
2O+O
2→ 4Fe (OH)
3↓ (two step precipitations)
Ni
2++OH
-→Ni(OH)
2↓
C, ammonia lixiviate nickel
Ni
2+6NH
3+CO
3 2-→Ni(NH
3)
6CO
3
D, acidifying
Ni(NH
3)
6CO
3+4H
2SO
4→NiSO
4+3(NH
4)
2SO
4+CO
2↑+H
2O
The preparation of e, nickelous carbonate
3Ni
2++4OH
-+CO
3 2-+4H
2O→NiCO
3·2Ni(OH)
2·4H
2O↓
F, nickelous carbonate acidolysis prepare single nickel salt
NiCO
3·2Ni(OH)
2·4H
2O+3H
2SO
4→3NiSO
4+CO
2↑+9H
2O
G, calcining
2α-FeO(OH)→Fe
2O
3+H
2O↑
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the inventive method can make in the serpentine useful component such as nickel, iron obtain fully effectively utilizing, and produces products such as the well sold and in short supply nickelous carbonate of the market requirement, single nickel salt and red iron oxide, and has obtained higher nickel, iron recovery.Wherein, nickelous carbonate purity counts 47.93% with nickel, yield 90.10%; Single nickel salt purity counts 22.12% with nickel, yield 85.73%; Red iron oxide purity is with Fe
2O
3Count 92.40%, yield 92.94%.
2, the present invention uses the ammonia soaking technology to carry out the purification of nickel, sink nickel with carbonate, effect is obvious, has improved the total yield of nickel, and avoids using halogenide as activator and sulfide for precipitation nickel may cause equipment material is had relatively high expectations and problem such as environmental pollution.
3, operational path used in the present invention has processing condition gentleness (normal pressure ,≤100 ℃), easy and simple to handle, advantage such as energy consumption is low, raw materials consumption is less, production cost is lower.
Four, embodiment
The present invention is further analyzed and described below in conjunction with embodiment.
Embodiment 1:
(1) pre-treatment: serpentine and mine tailing ore deposit thereof are carried out fragmentation, ore grinding, make the mineral aggregate granularity be not more than 75 μ m after the processing and obtain powder.
(2) acidleach: the sulphuric acid soln that in powder, adds mass concentration 30wt% with 4: 1 ratio of mass ratio, reacted 3 hours down at 95 ℃, reaction finishes after-filtration separated and collected filtrate and filter cake, filter cake is washed to neutrality with clear water obtain filter cake I, merges washings and filtrate and obtains filtrate I.Filtrate I collects and enters next step, and filter cake I collects and can be used for preparing the silicon series product.
(3) fractional precipitation: dropping ammonia regulation system pH value to 3.5 among the gained filtrate I in step 2, reacted 4 hours down in 70 ℃, reaction finishes after-filtration and separates filter cake and filtrate, filter cake is washed till neutrality with clear water obtains filter cake II, and merging filtrate and washings obtain filtrate II; Described filter cake II was the red iron oxide presoma after under 105 ℃ dry 4 hours, collect standby; Described filtrate II adds ammoniacal liquor regulation system pH value to 8, in 45 ℃ of down reactions 2 hours, after finishing, reaction continued under this temperature ageing 3 hours, filtering separation filter cake and filtrate, filter cake is washed till neutrality with clear water obtains filter cake III, merging filtrate and washings obtain filtrate II I.Filter cake III collection enters next step and handles, and filtrate II I can be used for preparing the magnesium series product.
(4) ammonia lixiviate nickel: in step 3 gained filter cake III, add the mixing solutions of ammoniacal liquor and bicarbonate of ammonia, NH in the mixing solutions of ammoniacal liquor and bicarbonate of ammonia in 4: 1 ratio of mass ratio
3Concentration 5mol/L, NH
4HCO
3Concentration 5mol/L, reacted 1.5 hours down at 70 ℃, reaction finishes after-filtration and collects filtrate and filter cake, filter cake extremely is back to step of acid dipping with obtaining filter cake IV behind the dimethylglyoxime solution detection non-nickle ion with the mixing solutions washing of ammoniacal liquor and bicarbonate of ammonia, and filtrate and washings merging obtain blue filtrate IV.
(5) acidifying: add sulfuric acid in step 4 gained filtrate IV the blueness of filtrate IV is taken off, destroy the nickel ammine structure, nickel is existed in solution with the ionic state form, the carbonic acid gas that reaction produces can be recycled after absorption is handled.
(6) preparation of nickelous carbonate: the pH value with the filtrate IV after the sodium carbonate solution adjusting acidifying of mass concentration 10wt% is 9, reacts 1.5 hours down at 80 ℃; Reaction finishes after-filtration and separates filter cake and filtrate, and filter cake is collected the back and was nickelous carbonate in dry 3.5 hours down at 108 ℃, and nickel content is 47.93% in the nickelous carbonate, has reached the requirement of quality standard, and the nickelous carbonate yield is 90.10%.Filtrate cycle is used.
(7) preparation of single nickel salt: with the nickelous carbonate that obtains in the step 6 sulfuric acid dissolution with mass concentration 10wt%, control reaction end pH is 3.5, and being concentrated into density is 1.2g/cm
3After, be cooled to room temperature, place for some time to allow its crystallization and filtration, with filter cake 35 ℃ dry 7 hours down, promptly obtain the single nickel salt product.Nickel content is 22.12% in this product, has reached the requirement of quality standard, and the single nickel salt yield is 85.73%.Filtrate cycle is used.
(8) calcining: step 3 gained red iron oxide presoma was calcined 1 hour down at 800 ℃, got the red iron oxide product.This product purity is with Fe
2O
3Count 92.40%, reached the requirement of quality standard, the red iron oxide yield is 92.94%.
Embodiment 2:
(1) pre-treatment: serpentine and mine tailing ore deposit thereof are carried out fragmentation, ore grinding, make the mineral aggregate granularity be not more than 106 μ m after the processing and obtain powder.
(2) acidleach: the sulphuric acid soln that in powder, adds mass concentration 48wt% with 2.5: 1 ratio of mass ratio, reacted 4 hours down at 80 ℃, reaction finishes after-filtration separated and collected filtrate and filter cake, filter cake is washed to neutrality with clear water obtain filter cake I, merges washings and filtrate and obtains filtrate I.Filtrate I collects and enters next step, and filter cake I collects and can be used for preparing the silicon series product.
(3) fractional precipitation: dropping ammonia regulation system pH value to 3.0 among the gained filtrate I in step 2, reacted 3 hours down in 90 ℃, reaction finishes after-filtration and separates filter cake and filtrate, filter cake is washed till neutrality with clear water obtains filter cake II, and merging filtrate and washings obtain filtrate II; Described filter cake II was the red iron oxide presoma after under 108 ℃ dry 3 hours, collect standby; Described filtrate II adds ammoniacal liquor regulation system pH value to 8.5, reaction is 4 hours under room temperature, continues under this temperature ageing after reaction finishes 6 hours, filtering separation filter cake and filtrate, filter cake is washed till neutrality with clear water obtains filter cake III, merging filtrate and washings obtain filtrate II I.Filter cake III collection enters next step and handles, and filtrate II I can be used for preparing the magnesium series product.
(4) ammonia lixiviate nickel: in step 3 gained filter cake III, add the mixing solutions of ammoniacal liquor and bicarbonate of ammonia, NH in the mixing solutions of ammoniacal liquor and bicarbonate of ammonia in 5: 1 ratio of mass ratio
3Concentration 4mol/L, NH
4HCO
3Concentration 4mol/L, reacted 0.5 hour down at 90 ℃, reaction finishes after-filtration and collects filtrate and filter cake, filter cake extremely is back to step of acid dipping with obtaining filter cake IV behind the dimethylglyoxime solution detection non-nickle ion with the mixing solutions washing of ammoniacal liquor and bicarbonate of ammonia, and filtrate and washings merging obtain blue filtrate IV.
(5) acidifying: add sulfuric acid in step 4 gained filtrate IV blueness is taken off, destroy the nickel ammine structure, nickel is existed in solution with the ionic state form, the carbonic acid gas that reaction produces can be recycled after absorption is handled.
(6) preparation of nickelous carbonate: the pH value with the filtrate IV after the sodium carbonate solution adjusting acidifying of mass concentration 5wt% is 8, reacts 0.5 hour down at 90 ℃; Reaction finishes after-filtration and separates filter cake and filtrate, and filter cake is collected the back and was nickelous carbonate in dry 2.5 hours down at 110 ℃, and nickel content is 47.51% in the nickelous carbonate, has reached the requirement of quality standard, and the nickelous carbonate yield is 90.06%.Filtrate cycle is used.
(7) preparation of single nickel salt: with the nickelous carbonate that obtains in the step 6 sulfuric acid dissolution with mass concentration 8wt%, control reaction end pH is 3.0, and being concentrated into density is 1.1g/cm
3After, be cooled to room temperature, place for some time to allow its crystallization and filtration, with filter cake 30 ℃ dry 10 hours down, promptly obtain the single nickel salt product.Nickel content is 21.8% in this product, has reached the requirement of quality standard, and the single nickel salt yield is 85.70%.Filtrate cycle is used.
(8) calcining: step 3 gained red iron oxide presoma was calcined 2 hours down at 700 ℃, got the red iron oxide product.This product purity is with Fe
2O
3Count 91.27%, reached the requirement of quality standard, the red iron oxide yield is 92.73%.
Embodiment 3:
(1) pre-treatment: serpentine and mine tailing ore deposit thereof are carried out fragmentation, ore grinding, make the mineral aggregate granularity be not more than 150 μ m after the processing and obtain powder.
(2) acidleach: the sulphuric acid soln that in powder, adds mass concentration 12wt% with 10: 1 ratio of mass ratio, reacted 5 hours down at 60 ℃, reaction finishes after-filtration separated and collected filtrate and filter cake, filter cake is washed to neutrality with clear water obtain filter cake I, merges washings and filtrate and obtains filtrate I.Filtrate I collects and enters next step, and filter cake I collects and can be used for preparing the silicon series product.
(3) fractional precipitation: dropping ammonia regulation system pH value to 4.0 among the gained filtrate I in step 2, reacted 5 hours down in 50 ℃, reaction finishes after-filtration and separates filter cake and filtrate, filter cake is washed till neutrality with clear water obtains filter cake II, and merging filtrate and washings obtain filtrate II; Described filter cake II was the red iron oxide presoma after under 110 ℃ dry 2 hours, collect standby; Described filtrate II adds ammoniacal liquor regulation system pH value to 7.2, in 35 ℃ of down reactions 3 hours, after finishing, reaction continued under this temperature ageing 4.5 hours, filtering separation filter cake and filtrate, filter cake is washed till neutrality with clear water obtains filter cake III, merging filtrate and washings obtain filtrate II I.Filter cake III collection enters next step and handles, and filtrate II I can be used for preparing the magnesium series product.
(4) ammonia lixiviate nickel: in step 3 gained filter cake III, add the mixing solutions of ammoniacal liquor and bicarbonate of ammonia, NH in the mixing solutions of ammoniacal liquor and bicarbonate of ammonia in 3: 1 ratio of mass ratio
3Concentration 6mol/L, NH
4HCO
3Concentration 6mol/L, at room temperature reacted 3 hours, react the end after-filtration and collect filtrate and filter cake, filter cake extremely is back to step of acid dipping with obtaining filter cake IV behind the dimethylglyoxime solution detection non-nickle ion with the mixing solutions washing of ammoniacal liquor and bicarbonate of ammonia, and filtrate and washings merging obtain blue filtrate IV.
(5) acidifying: add sulfuric acid in step 4 gained filtrate IV blueness is taken off, destroy the nickel ammine structure, nickel is existed in solution with the ionic state form, the carbonic acid gas that reaction produces can be recycled after absorption is handled.
(6) preparation of nickelous carbonate: the pH value with the filtrate IV after the sodium carbonate solution adjusting acidifying of mass concentration 15wt% is 9.5, at room temperature reacts 3 hours; Reaction finishes after-filtration and separates filter cake and filtrate, and filter cake is collected the back and was nickelous carbonate in dry 4 hours down at 105 ℃, and nickel content is 47.41% in the nickelous carbonate, has reached the requirement of quality standard, and the nickelous carbonate yield is 90.05%.Filtrate cycle is used.
(7) preparation of single nickel salt: with the nickelous carbonate that obtains in the step 6 sulfuric acid dissolution with mass concentration 5wt%, control reaction end pH is 4.0, and being concentrated into density is 1.3g/cm
3After, be cooled to room temperature, place for some time to allow its crystallization and filtration, with filter cake 40 ℃ dry 5 hours down, promptly obtain the single nickel salt product.Nickel content is 21.70% in this product, has reached the requirement of quality standard, and the single nickel salt yield is 85.67%.Filtrate cycle is used.
(8) calcining: step 3 gained red iron oxide presoma was calcined 3 hours down at 600 ℃, got the red iron oxide product.This product purity is with Fe
2O
3Count 89.50%, reached the requirement of quality standard, the red iron oxide yield is 92.67%.
Claims (1)
1. one kind by extracting the method prepare nickelous carbonate, single nickel salt and red iron oxide in serpentine and the mine tailing thereof, with serpentine and mine tailing thereof is raw material, comprise that pre-treatment, acidleach, fractional precipitation, ammonia soak, the preparation of the preparation of acidifying, nickelous carbonate, single nickel salt and calcine each unit process, it is characterized in that:
Described pre-treatment is serpentine and mine tailing thereof to be milled to particle diameter obtain powder less than 200 μ m;
Described acidleach is the sulphuric acid soln that adds powder quality 2-10 mass concentration 10-50wt% doubly in described powder, reacted 3-5 hour down at 60-100 ℃, filtering separation is collected filtrate and filter cake, described filter cake is washed with water to neutrality obtains the filter cake I, washings and the merging of described filtrate are obtained the filtrate I;
Described fractional precipitation is to add lye pH adjustment value 3.0-4.0 in described filtrate I, in 50-90 ℃ of reaction 3-5 hour, reaction finishes after-filtration separated and collected filtrate and filter cake, filter cake is washed with water to neutrality obtains the filter cake II, with washings and described filtrate merge the filtrate II; Described filter cake II obtained the red iron oxide presoma after under 105-110 ℃ dry 2-4 hour; In described filtrate II, add lye pH adjustment value 7.0-8.5, room temperature-45 ℃ following reaction 2-4 hour, the still aging 3-6 of preserving heat after reaction ends hour, filtering separation was collected filtrate and filter cake, filter cake washing is obtained the filter cake III to neutrality, merge washings and filtrate and obtain the filtrate III; Described alkali lye is selected from ammoniacal liquor, sodium hydroxide or potassium hydroxide;
It is to add described filter cake III quality 3-5 times the ammoniacal liquor and the mixing solutions of bicarbonate of ammonia in described filter cake III that described ammonia soaks, at room temperature-90 ℃ following reaction 0.5-3 hour, NH in the mixing solutions of described ammoniacal liquor and bicarbonate of ammonia
3Concentration 4-6mol/L, NH
4HCO
3Concentration 4-6mol/L; React and finish after-filtration collection filtrate and filter cake, the mixing solutions of filter cake with described ammoniacal liquor and bicarbonate of ammonia washed to obtaining the filter cake IV with dimethylglyoxime solution detection non-nickle ion, collect washings and filtrate and obtain the filtrate IV;
Described acidifying is to add sulfuric acid in described filtrate IV, and the vitriolic add-on is so that the blueness of filtrate IV is taken off is as the criterion;
The preparation of described nickelous carbonate is the pH to 8-9.5 that regulates the filtrate IV after the acidifying with the carbonate solution of mass concentration 5-15wt%, 70-90 ℃ of reaction 0.5-3 hour down, filter back gained filter cake 105-110 ℃ dry 2-4 hour down, promptly obtain nickelous carbonate; Described carbonate is selected from yellow soda ash or salt of wormwood;
The preparation of described single nickel salt is the sulphuric acid soln dissolving of the nickelous carbonate of preparation being used mass concentration 5-10wt%, and control reaction end pH value 3-4 is concentrated into density 1.1-1.3g/cm
3Postcooling leaves standstill after-filtration to room temperature, and the gained filter cake was descended dry 5-10 hour at 30-40 ℃, promptly obtains single nickel salt;
Described calcining is that described red iron oxide presoma was calcined 1-3 hour down in 600-800 ℃, promptly gets red iron oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210103812 CN102616867B (en) | 2012-04-11 | 2012-04-11 | Method for extracting and preparing nickel carbonate, nickel sulfate and red ferric oxide from serpentine and tailings thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210103812 CN102616867B (en) | 2012-04-11 | 2012-04-11 | Method for extracting and preparing nickel carbonate, nickel sulfate and red ferric oxide from serpentine and tailings thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102616867A CN102616867A (en) | 2012-08-01 |
| CN102616867B true CN102616867B (en) | 2013-07-31 |
Family
ID=46557153
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210103812 Active CN102616867B (en) | 2012-04-11 | 2012-04-11 | Method for extracting and preparing nickel carbonate, nickel sulfate and red ferric oxide from serpentine and tailings thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102616867B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103566937A (en) * | 2012-08-07 | 2014-02-12 | 中国石油化工股份有限公司 | Catalytic coal gasification catalyst and preparation method thereof |
| CN103274483B (en) * | 2013-06-06 | 2016-01-13 | 重庆莘然高分子材料有限公司 | The nickel recovery process of nickel coating strip waste liquid |
| CN105694539B (en) * | 2016-02-29 | 2018-05-08 | 中国科学院兰州化学物理研究所 | A kind of method that iron oxide red hybrid pigment is prepared using clay mineral |
| CN105970002B (en) * | 2016-05-31 | 2019-03-26 | 福安市康齐动力科技有限公司 | Utilize the method for nickel in tail gas recycle lateritic nickel ore |
| CN114058848A (en) * | 2021-10-09 | 2022-02-18 | 杭州逐真科技有限公司 | System and process for recovering copper, nickel, zinc, chromium and iron from electroplating sludge or other multi-metal mixture |
| CN115786602B (en) * | 2022-10-11 | 2024-04-09 | 中国恩菲工程技术有限公司 | Method for preparing hematite by using iron-aluminum slag |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2378721A1 (en) * | 2002-03-22 | 2003-09-22 | Nichromet Extraction Inc. | Metals recovery from serpentine ores |
| CN101250622A (en) * | 2008-04-07 | 2008-08-27 | 戴元宁 | Complete wet way comprehensive processing method for serpentine mine |
| CN101525690A (en) * | 2009-04-15 | 2009-09-09 | 广西冶金研究院 | Method for separating and recovering nickel, cobalt, magnesium, iron and silicon from nickel-bearing laterite |
| CN102010986A (en) * | 2010-12-13 | 2011-04-13 | 昆明理工大学 | New process for comprehensively recovering serpentine type minerals |
-
2012
- 2012-04-11 CN CN 201210103812 patent/CN102616867B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2378721A1 (en) * | 2002-03-22 | 2003-09-22 | Nichromet Extraction Inc. | Metals recovery from serpentine ores |
| CN101250622A (en) * | 2008-04-07 | 2008-08-27 | 戴元宁 | Complete wet way comprehensive processing method for serpentine mine |
| CN101525690A (en) * | 2009-04-15 | 2009-09-09 | 广西冶金研究院 | Method for separating and recovering nickel, cobalt, magnesium, iron and silicon from nickel-bearing laterite |
| CN102010986A (en) * | 2010-12-13 | 2011-04-13 | 昆明理工大学 | New process for comprehensively recovering serpentine type minerals |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102616867A (en) | 2012-08-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102616867B (en) | Method for extracting and preparing nickel carbonate, nickel sulfate and red ferric oxide from serpentine and tailings thereof | |
| CN103667710B (en) | Technology for clean production of vanadium pentoxide employing high-calcium vanadium slag | |
| CN102329964B (en) | Method for separating and recovering vanadium and chromium from vanadium-chromium reduced waste residue | |
| CN100469697C (en) | Method for producing low-magnesium battery-stage lithium carbonate from lithium sulfate solution | |
| CN103395796B (en) | Comprehensive utilization method of serpentine and device used by method | |
| CN101235440A (en) | Method of comprehensively utilizing serpentine | |
| CN101723458B (en) | Method for cleanly extracting vanadium pentexide from vanadium containing material | |
| CN101760641B (en) | Technology for recovering magnesium from magnesium sulfate solution | |
| CN109666796B (en) | Recovery method of vanadium-containing neutralization slag | |
| CN101450811A (en) | Method for extracting alumina from coal gangue | |
| CN102070198A (en) | Method for preparing high-purity manganese sulfate and high-purity manganese carbonate by reduction leaching of pyrolusite through scrap iron | |
| CN101525143A (en) | Method for preparing magnesia, silicon dioxide and nickel oxide products from lateritic nickel ore | |
| CN102634673A (en) | Method for deeply removing iron ions from chromium-containing waste residue pickle liquor | |
| CN106611841A (en) | Method for preparing nickel-cobalt-manganese ternary material precursor by using nickel-cobalt slag material | |
| CN101693543B (en) | High value-added greening comprehensive utilization method of boron concentrate, boron-containing iron concentrate and ludwigite | |
| CN103101935A (en) | Method for preparing lithium carbonate from coal ash | |
| CN104760980B (en) | A kind of preparation technology of high-purity superfine alumina powder | |
| CN102923764A (en) | Method for preparing sodium stannate from stannic oxide and sodium salt in reduction roasting manner | |
| CN104760979A (en) | Preparation technology of highly pure alumina powder | |
| CN109319792A (en) | A kind of method that high added value comprehensively utilizes silicon, aluminium, potassium in potash feldspar ore | |
| CN109336147A (en) | A kind of method of the salic Industrial Solid Waste production aluminium oxide of richness | |
| CN101830475A (en) | Method for preparing magnesium silicate and magnesium hydroxide from serpentine or tailings thereof | |
| CN109384254A (en) | The method that crystal aluminum chloride and white carbon black are prepared by flyash or gangue | |
| CN101607721B (en) | Method for preparing highly pure magnesium hydroxide and magnesium hexa-silicate by using olivine tailing mine | |
| CN103910366A (en) | Method for preparing high-purity magnesium oxide by utilizing serpentinite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |